Ethanol → Bis(eta-cyclopentadienyl) iron

HRID 232109

반응식

HRID 232109 반응식
[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2].[Fe:12](Cl)([Cl:14])[Cl:13].C(O)C>CCOCC>[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2:12].[Fe:12]([Cl:14])[Cl:13]

참가 물질

6

반응물 3

HCID 702EthanolHCID 7611Bis(eta-cyclopentadienyl) ironHCID 24380Iron chloride (FeCl3)

생성물 2

HCID 7611Bis(eta-cyclopentadienyl) ironHCID 24458Ferrous Chloride

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Impure ferricenium tetrachloroferrate is prepared from ferrocene (2 mmol) and anhydrous iron(III) chloride (4 mmol) in ether, with recrystallization from absolute ethanol, by the process of Nesmeyanov et al. The product obtained, the infrared spectrum of which shows that it is a product contaminated with diferricenium μ-oxo-bis(trichloroferrate), can be recrystallized either from freshly distilled thionyl chloride or from 0.15-0.25M aqueous-methanolic (2:98) hydrogen chloride, a ferricenium tetrachloroferrate which is pure according to spectroscopy (disappearance of the maxima at 365 and 316 cm-1) and elemental analysis being obtained in the form of blue-black crystal flakes. Found: C, 31.22; H, 2.71; Cl, 36.80. Calculated for C10H10Cl4Fe2 : C, 31.30; H, 2.63; Cl, 36.96. The recrystallization from the acid medium can also be carried out directly with the crude product obtained from ferrocene and iron chloride, by-avoiding the recrystallization from absolute ethanol.

후처리

  1. customobtained
  2. customcan be recrystallized either from freshly distilled thionyl chloride or from 0.15-0.25M aqueous-methanolic (2:98) hydrogen chloride
  3. custombeing obtained in the form of blue-black crystal flakes
  4. customThe recrystallization from the acid medium

출처 및 근거

ORD 기록
ord-addad72e6a94407f99e85273bd235b03
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851430

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